Water-based environment-friendly halogen-free flame retardant and preparation method thereof

Through step-by-step mixing and directional flow grinding, the problem of unreasonable halogen-free flame retardant formulation is solved, and an efficient and low-cost preparation process is achieved, and product quality and production efficiency are improved.

CN120535783AInactive Publication Date: 2025-08-26ZHEJIANG DEJIU NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202510674408.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-23
Publication Date
2025-08-26
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing halogen-free flame retardant formula is unreasonable, resulting in complex preparation process, low efficiency, high cost and unenvironmental protection, making it difficult to expand production.

Method used

By setting up processing and mixing processes, the solid raw materials are first fully mixed and dispersed in water to avoid agglomeration and agglomeration, and then adding acrylic emulsion and thickener, and directional flow grinding and bubble removal are used to ensure the stability and uniformity of the emulsion.

Benefits of technology

It realizes efficient and low-cost halogen-free flame retardant preparation, suitable for mass production, stable product quality, and good flame retardant performance.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of combustion improvers, in particular to a water-based environment-friendly halogen-free flame retardant and a preparation method thereof. The preparation method of the flame retardant comprises the following steps: a treatment process: adding decabromodiphenyl ethane, antimony trioxide, ammonium polyphosphate, titanium dioxide and water into a mixing container, fully mixing, and pretreating to form a pretreatment solution; a mixing process: adding an acrylic emulsion and a thickening agent into the treatment solution in the mixing container, and fully mixing to form a halogen-free flame retardant; an inspection procedure: sampling the formed halogen-free flame retardant in the mixing container for multiple times, and inspecting whether the combustion effect of the sample is qualified after inspecting whether the sample contains unmixed large particles; and a packaging process: sub-packaging and packaging the qualified halogen-free flame retardant in the mixing container. The invention solves the problems of low preparation efficiency, difficulty in expanded production, high cost and no environmental protection caused by unreasonable formula of the existing halogen-free flame retardant.
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Description

Technical Field

[0001] The present invention relates to the technical field of combustion aids, and in particular to a water-based, environment-friendly, halogen-free flame retardant and a preparation method thereof. Background Art

[0002] With the improvement of the national economic level and the development of science and technology, polymer materials represented by plastic products, rubber products and fiber products have been widely used in daily life. Since polymer materials themselves are extremely flammable, they need to be used in combination with a flame retardant that can effectively prevent combustion and inhibit the spread of combustion flames, so that the flammable polymer materials can obtain functional additives with flame-retardant properties. At present, halogen-containing flame retardants have a large share in organic flame retardant systems due to their good compatibility and high cost performance. However, halogen-containing flame retardants produce toxic and harmful gases accompanied by thick smoke when heated, which seriously affects people's life and health as well as the natural environment. Therefore, research on halogen-free flame retardants has become a hot direction for the current research and development of flame retardant technology. Whether from the technical field or the environmental protection direction, high-efficiency, energy-saving and environmentally friendly halogen-free flame retardants are the future research and development focus of the flame retardant industry.

[0003] Patent document CN112876739A discloses a method for preparing a halogen-free flame retardant, a halogen-free flame retardant, and a sealant. The method comprises: adding an ethanol solution of piperazine pyrophosphate and a layered inorganic compound to a melamine-formaldehyde resin; adjusting the pH of the system to 3-5; and conducting a hydrothermal reaction at 65-85°C for 3-5 hours to obtain a mixed coated reactant, wherein the mass ratio of the melamine-formaldehyde resin, the ethanol solution of piperazine pyrophosphate, and the layered inorganic compound is 0.5-0.9:2:0.7-1.1; and uniformly spraying a surface modifier, prepared by mixing a vinyl silane coupling agent, vinyl silicone oil, and hydroxyl silicone oil at 115-130°C for 65-85 minutes, into the mixed coated reactant to perform a surface coupling treatment to obtain the halogen-free flame retardant. The halogen-free flame retardant obtained by the present invention exhibits strong compatibility and good dispersion when mixed with the sealant system. Even a small amount of addition can impart excellent flame retardancy to the sealant and significantly improve smoke suppression performance.

[0004] However, during the actual production process, the inventors found that the formula of the existing halogen-free flame retardants was unreasonable during preparation, which made the preparation conditions relatively harsh and difficult to achieve large-scale production. In addition, the preparation process was relatively complicated and unreasonable, and the preparation time was long, which greatly affected the production efficiency. In addition, the preparation process required the use of a large amount of organic solvents, which was costly and not environmentally friendly. Summary of the Invention

[0005] The present invention aims to address the deficiencies of the prior art. By setting a treatment process and a mixing process, the present invention achieves step-by-step mixing during production. First, solid raw material components of decabromodiphenylethane, antimony trioxide, ammonium polyphosphate and titanium dioxide are fully mixed and dispersed in water to avoid agglomeration and agglomeration. Then, an acrylic emulsion and a thickener are added to prevent the destruction of polymer chains and maintain the stability of the emulsion. The entire production process of the halogen-free flame retardant product is a physical reaction, and production can be carried out by uniform stirring under normal temperature conditions. Thus, the problems of the existing halogen-free flame retardant due to unreasonable formulation, low preparation efficiency, difficulty in scaled-up production, high cost and environmental pollution are solved.

[0006] In response to the above technical problems, the following technical solutions are adopted: A method for preparing a water-based environmentally friendly halogen-free flame retardant, comprising the following steps: Step 1: A treatment process in which raw materials, decabromodiphenylethane, antimony trioxide, ammonium polyphosphate, titanium dioxide, and water are added to a mixing mechanism to form a mixture A. The mixing mechanism guides the mixture A to flow in a directional manner while stirring the mixture A for grinding until the solid raw materials are fully ground and mixed into the water to form a pretreatment solution. Step 2: Mixing process, adding the raw acrylic emulsion and the thickener to the pretreatment solution in the mixing mechanism to form a mixture B, and the mixing mechanism guides the mixture B to flow in a directional manner for grinding while stirring the mixture B. During the grinding process, the mixing mechanism further guides the mixture B to flow in a directional manner to collect and remove bubbles until the solid raw material is fully ground and mixed into the pretreatment solution and the bubbles are completely collected and removed to form a halogen-free flame retardant.

[0007] Preferably, the mixing mechanism includes a mixing tank with an open upper end, a grinding assembly arranged in the mixing tank, a defoaming assembly arranged on the grinding assembly, and a stirring assembly rotatably arranged in the mixing tank, and the stirring assembly is used to guide the solution on both sides of the mixing tank to the grinding assembly.

[0008] Preferably, the grinding assembly includes a support frame arranged in the mixing tank, two rotating rollers that are spaced apart and rotatably arranged on the support frame and form a first grinding zone between the two, two grinding rollers that are rotatably arranged on the support frame and respectively cooperate with the two rotating rollers to form two second grinding zones, and two guide plates that are opened and closed on the support frame and located between the two rotating rollers, and the guide plates are used to further guide the solution on the inside and outside of the mixing tank guided by the stirring assembly into the two second grinding zones or the first grinding zone by opening or closing.

[0009] Preferably, the debubble component includes a debubble channel formed through the rotating roller and the grinding roller, a screen arranged at the lower end of the debubble channel, a spiral plate arranged in the debubble channel, and a plurality of inflow holes arranged at the upper ends of the rotating roller and the grinding roller and extending through the corresponding debubble channels, and the spiral plate is used to further guide the solution to flow to the screen to collect and remove bubbles while the rotating roller cooperates with the grinding roller to grind.

[0010] Preferably, in the treatment process, the mixing mechanism first stirs at a low speed to preliminarily dissolve the solid raw material in water to form a mixture A, then stirs at a high speed to increase the grinding speed of the solid raw material in the mixture A, and finally stirs at a low speed to naturally expel the bubbles that are quickly stirred into the mixture A to form a pretreatment solution; In the mixing process, the mixing mechanism first stirs at a low speed to preliminarily dissolve the solid raw materials into the pretreatment solution to form a mixture B, then stirs at a high speed to increase the grinding speed of the solid raw materials in the mixture B, and finally stirs at a low speed to directionally collect and remove the bubbles that are quickly stirred into the mixture B to form a halogen-free flame retardant.

[0011] Preferably, the method for preparing the water-based environmentally friendly halogen-free flame retardant further comprises the following steps: Step 3: Inspection process, sampling the halogen-free flame retardant formed in the mixing mechanism multiple times, and after inspecting whether the sample contains unmixed large particles, inspecting whether the combustion effect of the sample is qualified; Step 4: packaging process, the halogen-free flame retardant that has passed the inspection in the mixing mechanism is packaged.

[0012] Preferably, in the inspection process, qualified inspection values ​​of flame temperature and oxygen content are set to inspect whether the halogen-free flame retardant continues to burn.

[0013] Preferably, in the inspection process, the flame temperature and oxygen content are increased to allow the halogen-free flame retardant to burn out continuously, and whether the carbon film produced after the combustion of the halogen-free flame retardant is dense and continuous is detected.

[0014] The present application also provides a flame retardant obtained by the above-mentioned method for preparing a water-based environmentally friendly halogen-free flame retardant, comprising: 12% decabromodiphenylethane, 4% antimony trioxide, 8% ammonium polyphosphate, 4% titanium dioxide, 30% acrylic emulsion, 2% thickener and 40% water.

[0015] Preferably, the thickener is bentonite, magnesium aluminum silicate, hydroxyethyl cellulose or carboxymethyl cellulose.

[0016] Beneficial effects of the present invention: (1) In the present invention, by setting up a treatment process and a mixing process, step-by-step mixing is achieved during production. First, the solid raw material components are fully mixed and dispersed in water to form a pretreatment solution, so as to avoid agglomeration and agglomeration when directly added to the emulsion, thereby ensuring the uniformity of distribution of each component during the distribution and mixing process, and facilitating the preliminary mixing of decabromodiphenylethane and antimony trioxide in the pretreatment to form a bromine-antimony synergistic flame retardant mechanism. Then, the acrylic emulsion and the thickener are added and fully mixed and dispersed in the pretreatment solution to form a halogen-free flame retardant, thereby preventing the destruction of the polymer chain and maintaining the stability of the emulsion.

[0017] (2) The special structural setting of the mixing mechanism in the present invention changes the state of the mixture that originally moves irregularly, whether in the processing process or in the mixing process. That is, through the guidance of the effective structure, the mixture A and the mixture B are ground in a directional process, which is highly targeted and improves the efficiency of breaking up agglomerates, further improving the mixing efficiency. In the grinding process, the mixture A and the mixture B are further guided to flow in a directional manner to collect and remove bubbles, which facilitates the collection of bubbles, improves the efficiency of bubble removal, and further improves the quality and stability of the product. (3) In the present invention, decabromodiphenylethane, antimony trioxide, ammonium polyphosphate, titanium dioxide, acrylic emulsion and thickener are mixed and dissolved in water. The product produced by this formula is a physical reaction, with a reasonable formula, high preparation efficiency and convenience for mass production. It only needs to reasonably add raw materials and stir evenly under room temperature conditions to carry out production. It has low cost and environmental protection effects. In addition, decabromodiphenylethane forms a gas phase flame retardant to interrupt the combustion chain reaction, ammonium polyphosphate condensed phase flame retardant, promotes carbonization and heat insulation, antimony trioxide and bromine series synergistic effect, greatly improving the flame retardant efficiency, titanium dioxide has both flame retardant auxiliary and covering properties, and the four synergistically combine to improve the flame retardant effect; In summary, the halogen-free flame retardant in this application has a reasonable formula, high preparation efficiency, is easy to mass produce, low cost and environmentally friendly, and is particularly suitable for the field of flame retardant technology. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0019] Figure 1 This is a preparation flow chart of a method for preparing a water-based, environmentally friendly, halogen-free flame retardant provided by the present invention.

[0020] Figure 2 This is a three-dimensional diagram of a flame retardant preparation device provided by the present invention.

[0021] Figure 3 A three-dimensional cross-sectional view of the mixing mechanism provided by the present invention.

[0022] Figure 4 The present invention provides Figure 3 A partial enlarged view of point A in the middle.

[0023] Figure 5 A side view of the mixing mechanism provided by the present invention.

[0024] Figure 6 The present invention provides Figure 5 Cross-sectional view along the middle edge B.

[0025] Figure 7 The present invention provides Figure 5 Cross-sectional view along the center line C.

[0026] Figure 8 When the first grinding zone provided by the present invention grinds raw materials Figure 7 Schematic diagram of the structure.

[0027] Figure 9 When the second grinding zone provided by the present invention grinds raw materials Figure 7 Schematic diagram of the structure.

[0028] Figure 10 A three-dimensional cross-sectional view of the inspection mechanism provided by the present invention.

[0029] Figure 11 The present invention provides Figure 10 A partial enlarged view of point D in the middle. DETAILED DESCRIPTION

[0030] The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the accompanying drawings.

[0031] Example 1 like Figure 1-Figure 2 As shown, a method for preparing a water-based environmentally friendly halogen-free flame retardant comprises the following steps: Step 1: Treatment process: raw materials decabromodiphenylethane, antimony trioxide, ammonium polyphosphate, titanium dioxide and water are added to the mixing mechanism 1 to form a mixture A. The mixing mechanism 1 guides the mixture A to flow in a directional manner while stirring the mixture A for grinding until the solid raw materials are fully ground and mixed into the water to form a pretreatment solution; Step 2: Mixing process, adding the raw acrylic emulsion and thickener to the pretreatment solution in the mixing mechanism 1 to form a mixture B, the mixing mechanism 1 guides the mixture B to flow in a directional manner while stirring the mixture B for grinding, and during the grinding process, the mixing mechanism 1 further guides the mixture B to flow in a directional manner to collect and remove bubbles, until the solid raw material is fully ground and mixed into the pretreatment solution and the bubbles are completely collected and removed, thereby forming a halogen-free flame retardant.

[0032] In this embodiment, by setting up a treatment process and a mixing process, step-by-step mixing is achieved during production. The solid raw material components are first fully mixed and dispersed in water to avoid caking and agglomeration when directly added to the emulsion, thereby ensuring the uniformity of distribution of each component during the distribution mixing process. Then, the acrylic emulsion and the thickener are added to prevent the destruction of the polymer chain and maintain the stability of the emulsion. During the mixing process, the mixture A and the mixture B are guided to grind, thereby improving the efficiency of breaking the agglomerates and further improving the mixing efficiency. During the grinding process, the mixture A and the mixture B are further guided to flow in a directional manner to collect and remove bubbles, thereby facilitating the collection of bubbles, improving the efficiency of bubble removal, and further improving the quality and stability of the product.

[0033] Further, if Figure 1-Figure 3 As shown, in the treatment process, the mixing mechanism 1 first stirs at a low speed to preliminarily dissolve the solid raw materials into water to form a mixture A, then stirs at a high speed to increase the grinding speed of the solid raw materials in the mixture A, and finally stirs at a low speed to naturally expel the bubbles that have been stirred into the mixture A to form a pre-treated solution; In the mixing process, the mixing mechanism 1 first stirs at a low speed to initially dissolve the solid raw materials into the pretreatment solution to form a mixture B, then stirs at a high speed to increase the grinding speed of the solid raw materials in the mixture B, and finally stirs at a low speed to directionally collect and remove the bubbles that are quickly stirred into the mixture B to form a halogen-free flame retardant.

[0034] In this embodiment, by setting the stirring speed of the mixing mechanism 1 to low speed stirring at the beginning, the raw materials are gradually moistened and preliminarily mixed, avoiding dust or agglomeration of the powder raw materials and agglomeration of the emulsion. High-speed stirring is used in the middle stage to quickly break up the undispersed agglomerates, improve the mixing efficiency, achieve good mixing effect, ensure the uniformity of the mixed dispersion, and improve the product quality. Low-speed stirring is used in the later stage to facilitate the floating and escape of tiny bubbles and their collection and removal, thereby improving the product quality and stability.

[0035] Further, if Figure 1-Figure 2 As shown, the preparation method of the water-based environmentally friendly halogen-free flame retardant further includes the following steps: Step 3: Inspection process, sampling the halogen-free flame retardant formed in the mixing mechanism 1 multiple times, and after checking whether the sample contains unmixed large particles, inspecting whether the combustion effect of the sample is qualified; Step 4: Packaging process, the halogen-free flame retardant that has passed the inspection in the mixing mechanism 1 is packaged.

[0036] In this embodiment, by setting up an inspection process and a packaging process, the halogen-free flame retardant that has passed the inspection is packaged and divided into packages, and double verification is carried out through particle size detection and combustion test to ensure product consistency and facilitate the feasibility of product automation and industrialization.

[0037] Further, if Figure 1 As shown, during the inspection process, qualified inspection values ​​of flame temperature and oxygen content are set to inspect whether the halogen-free flame retardant continues to burn.

[0038] Further, if Figure 1 As shown, during the inspection process, the flame temperature and oxygen content are increased to allow the halogen-free flame retardant to continuously burn out, and the carbon film produced after the combustion of the halogen-free flame retardant is tested to see whether it is dense and continuous.

[0039] Example 2 A flame retardant, obtained by the method for preparing a water-based, environmentally friendly, halogen-free flame retardant in Example 1, comprising: 12% decabromodiphenylethane, 4% antimony trioxide, 8% ammonium polyphosphate, 4% titanium dioxide, 30% acrylic emulsion, 2% thickener and 40% water.

[0040] In this embodiment, the product produced by this formula is a physical reaction with a reasonable formula, high preparation efficiency, and easy mass production. It only needs to reasonably add raw materials and stir evenly at room temperature to carry out production. It has low cost and environmental protection effects. Decabromodiphenylethane forms a gas phase flame retardant, interrupting the combustion chain reaction, ammonium polyphosphate condensed phase flame retardant, promoting carbonization and heat insulation, antimony trioxide and bromine series synergistic effect, greatly improving the flame retardant efficiency, titanium dioxide has both flame retardant auxiliary and covering properties, and the four are combined synergistically to improve the flame retardant effect.

[0041] Furthermore, the thickener is bentonite, magnesium aluminum silicate, hydroxyethyl cellulose or carboxymethyl cellulose.

[0042] In this embodiment, the thickener is of natural or semi-natural origin and is relatively safe. Compared with some synthetic thickeners, these four raw materials are moderately priced and suitable for industrial production. They also have good water solubility and water dispersibility, good chemical stability, and a certain tolerance to general acid, alkali and salt chemicals.

[0043] Example 3 like Figure 1-Figure 3 As shown, a flame retardant preparation device, based on a method for preparing a water-based environmentally friendly halogen-free flame retardant in Example 1, comprises: A mixing mechanism 1 for mixing halogen-free flame retardants, a feeding mechanism 2, an inspection mechanism 3, and a packaging mechanism 4 are arranged outside the mixing mechanism 1. The feeding mechanism 2 is used to fill raw materials into the mixing mechanism 1. The inspection mechanism 3 is used to inspect the halogen-free flame retardants mixed in the mixing mechanism 1. The packaging mechanism 4 is used to package and pack qualified halogen-free flame retardants in the mixing mechanism 1. The mixing mechanism 1 includes a frame 11 rotatably arranged on the feeding mechanism 2, two mixing tanks 12 arranged on the frame 11 and having an open upper end 121, a grinding assembly 13 arranged in the mixing tank 12 and used for grinding the raw material, a defoaming assembly 14 arranged on the grinding assembly 13 and used for removing bubbles in the halogen-free flame retardant in the mixing tank 12, and a stirring assembly 15 rotatably arranged in the mixing tank 12 and used for stirring the raw material while guiding the raw material to move toward the grinding assembly 13.

[0044] In this embodiment, two mixing tanks 12 are provided to cooperate with the feeding mechanism 2 to feed materials alternately, and the stirring component 15, the grinding component 13 and the defoaming component 14 are cooperated to realize continuous production, improve production capacity, improve product quality, carry out the processing process and the mixing process simultaneously, reduce downtime, and the stirred halogen-free flame retardant is assisted by the inspection mechanism 3 and the packaging mechanism 4 to package and pack the halogen-free flame retardant that has passed the inspection, realize the inspection process and the packaging process, and realize automatic continuous and industrialized production of the product.

[0045] In detail, when in use, the feeding mechanism 2 adds the raw materials required for the treatment process into a mixing tank 12 and cooperates with the stirring component 15 to mix them into a pretreatment solution, and cooperates with the grinding component 13 and the defoaming component 14 to break up the agglomerates and collect and remove the bubbles; then the mixing tank 12 is rotated and the raw materials required for the mixing process are added to the pretreatment solution of the mixing tank 12 through the feeding mechanism 2 to mix them into a halogen-free flame retardant, and cooperates with the grinding component 13 and the defoaming component 14 to break up the agglomerates and collect and remove the bubbles. At this time, the feeding mechanism 2 adds the raw materials required for the treatment process into another mixing tank 12 and simultaneously performs the treatment process and the mixing process; then the halogen-free flame retardant that has passed the inspection by the inspection mechanism 3 is packaged and packed through the packaging mechanism 4; finally, before the mixing tank 12 that has completed the packaging and packing is rotated for the next round of production, the feeding mechanism 2 sprays a high-pressure water flow to clean the mixing tank 12 to avoid affecting the next round of production.

[0046] It should be noted that the feeding mechanism 2 for automatic proportioning and conveying of raw materials is a prior art and will not be described in detail here.

[0047] Further, if Figure 3As shown, the stirring assembly 15 includes a stirring rod 151 rotatably set on the frame 11 and with the lower end extending into the mixing tank 12, a plurality of first stirring blades 152 arranged at intervals on the stirring rod 151 and stirring the raw materials to flow toward the outside of the mixing tank 12, a plurality of extension rods 153 arranged at intervals on the stirring rod 151 and extending toward the outside of the mixing tank 12, a second stirring blade 154 movably set at one end of the extension rod 153 away from the stirring rod 151 and stirring the raw materials to flow toward the inside of the mixing tank 12, and a first elastic member 155 arranged on the extension rod 153 and used to force the second stirring blade 154 to move toward the inside of the mixing tank 12.

[0048] In this embodiment, the first stirring blade 152 and the second stirring blade 154 are provided to move the raw materials toward the grinding assembly 13 while stirring. At the same time, the first elastic member 155 is used to cooperate with the rotation speed of the stirring rod to control the movement of the second stirring blade 154, so that the second stirring blade 154 can scrape the raw materials on the inner wall of the mixing tank 12, thereby improving the stirring effect, reducing the time of high-speed rotation, reducing bubbles in the solution, and facilitating the cleaning of the mixing tank 12, while avoiding the second stirring blade 154 always contacting the inner wall of the mixing tank 12, affecting the service life of the device.

[0049] In detail, when the stirring rod 151 rotates, the first stirring blade 152 and the second stirring blade 154 respectively stir the raw materials to flow to the outside or inside of the mixing tank 12 to the grinding assembly 13 for grinding and defoaming; when the stirring rod 151 rotates at high speed, under the action of the increasing centrifugal force, the second stirring blade 154 moves outward until it abuts against the inner wall of the mixing tank 12, scraping off the raw materials attached to the inner wall of the mixing tank 12 and guiding the flow, at this time the first elastic member 155 is deformed; when the stirring rod 151 rotates at low speed, the centrifugal force becomes smaller, and the first elastic member 155 restores its deformation, forcing the second stirring blade 154 to move inward directly out of the mixing tank 12.

[0050] It should be noted that the first stirring blade 152 and the second stirring blade 154 are both spiral structures, and the spiral directions of the two are opposite, which makes the stirring raw materials have a certain circular motion in the up and down directions during the stirring process, further improving the stirring effect and efficiency.

[0051] Further, if Figure 4-Figure 9As shown, the grinding assembly 13 includes a support frame 131 arranged in the mixing tank 12 and located between the first stirring blade 152 and the second stirring blade 154, two rotating rollers 132 that are spaced apart and rotatably arranged on the support frame 131 and form a first grinding area 133 therebetween, two grinding rollers 134 that are rotatably arranged on the support frame 131 and respectively cooperate with the two rotating rollers 132 to form two second grinding areas 135, and two guide plates 136 that are opened and closed on the support frame 131 and located between the two rotating rollers 132, and the guide plates 136 are used to guide the raw materials stirred by the first stirring blade 152 and the second stirring blade 154 into the two second grinding areas 135 or the first grinding area 133 by opening or closing.

[0052] In this embodiment, by providing a rotating roller 132 in conjunction with the grinding roller 134 and the guide plate 136, the first stirring blade 152 and the second stirring blade 154 can stir the large particles of raw materials and guide them to the first grinding area 133 for preliminary grinding into small particles, and then stir the small particles and guide them to the second grinding area 135 for precision grinding, thereby improving the grinding effect.

[0053] In detail, when in use, the first stirring blade 152 and the second stirring blade 154 have a certain stirring and guiding direction for the raw material; when performing preliminary grinding, the two guide plates 136 are closed to guide the raw material stirred by the first stirring blade 152 and the second stirring blade 154 into the first grinding zone 133 respectively. At this time, based on the first grinding zone 133, the rotation direction of the rotating roller 132 is consistent with the flow direction of the raw material, which is convenient for preliminary grinding of the raw material. At the same time, based on the second grinding zone 135, the rotation direction of the grinding roller 134 is opposite to the flow direction of the raw material, which prevents large particles of raw material from flowing into and being retained in the second grinding zone 135, affecting the preliminary grinding efficiency; when performing precision grinding, the two guide plates 136 are opened to block the first grinding zone 133 while guiding the raw material stirred by the first stirring blade 152 and the second stirring blade 154 into the two second grinding zones 135 respectively. At this time, based on the second grinding zone 135, the rotation directions of the rotating roller 132 and the grinding roller 134 are the same as the flow direction of the raw material, achieving fine grinding.

[0054] It should be noted that there are multiple grinding assemblies 13 to improve grinding efficiency.

[0055] Further, if Figure 4-Figure 9 As shown, the defoaming component 14 includes a defoaming channel 141 formed through the rotating roller 132 and the grinding roller 134, a screen 142 arranged at the lower end of the defoaming channel 141, a spiral plate 143 arranged in the defoaming channel 141, and a plurality of inflow holes 144 arranged at the upper ends of the rotating roller 132 and the grinding roller 134 and extending through the corresponding defoaming channels 141.

[0056] In this embodiment, a spiral plate 143 is provided to guide the solution in the mixing tank 12 to the screen 142 through the debubbling channel 141 during the grinding process, so as to collect and remove bubbles. At the same time, the inflow hole 144 is used to increase the speed at which the solution flows into the debubbling channel 141, thereby increasing the debubbling speed and the production speed.

[0057] In detail, during the initial grinding, the spiral plate 143 rotates with the rotating roller 132 and the grinding roller 134 to force the raw materials in the debubble channel 141 to move away from the screen 142, thereby preventing large particles of raw materials from accumulating in the debubble channel 141; during the precision grinding, the spiral plate 143 rotates in the opposite direction with the rotating roller 132 and the grinding roller 134, thereby forcing the raw materials to move toward the screen 142 through the inflow hole 144 and the debubble channel 141, small particles and solution are able to pass through the screen 142, and small bubbles are able to be intercepted by the screen 142 until the small bubbles merge with the large bubbles and slowly float out of the debubble channel 141 and then float out of the solution.

[0058] It should be noted that the screen 142 is a conical structure protruding outward from the defoaming channel 141. During the non-defoaming period, it can guide the solution containing large particle raw materials to flow toward the sides of the rotating roller 132 and the grinding roller 134 to avoid clogging of the screen 142.

[0059] Further, if Figure 2-Figure 3 as well as Figure 10-11 As shown, the inspection mechanism 3 includes a discharge port 31 formed at the bottom of the mixing tank 12 and capable of being opened and closed, an inspection bin 32 arranged on the outside of the feeding mechanism 2 and capable of being opened and closed, a movable frame 33 movable and rotatable between the discharge port 31 and the inspection bin 32, a plurality of inspection plates 34 spaced apart on the movable frame 33 and used for carrying halogen-free flame retardants, a scraping assembly 35 arranged in the inspection bin 32 and used for scraping and inspecting the halogen-free flame retardants, and a combustion assembly 36 arranged in the inspection bin 32 and used for burning and inspecting the halogen-free flame retardants.

[0060] In this embodiment, a movable rack 33 is provided to cooperate with a plurality of inspection trays 34 to transport a plurality of samples drawn out from the discharge port 31 into the inspection chamber 32, and then a scraping assembly 35 and a combustion assembly 36 are used to inspect each sample.

[0061] Further, if Figure 2-Figure 3 as well as Figure 10-11 As shown, the scraping assembly 35 includes a mounting frame 351 arranged in the inspection chamber 32, a scraper 352 rotatably arranged on the mounting frame 351, a second elastic member 353 arranged on the mounting frame 351 and used to force one end of the scraper 352 to abut against the inspection disk 34, and a sensor 354 arranged on the scraper 352 and used to detect pressure changes on the second elastic member 353.

[0062] In this embodiment, a scraper 352 is provided to cooperate with the second elastic member 353 to scrape the halogen-free flame retardant on the inspection disk 34, and is detected in cooperation with the sensor 354. When the halogen-free flame retardant contains large particles of raw materials, the scraper 352 rotates upward to force the second elastic member 353 to deform, and the pressure detected by the sensor 354 increases.

[0063] It should be noted that the first elastic member 155 and the second elastic member 353 can be coil springs, leaf springs, etc. The first elastic member 155, the second elastic member 353 and the sensor 354 themselves and their installation methods are all existing technologies and will not be described in detail here.

[0064] Further, if Figure 2-Figure 3 As shown, the combustion assembly 36 includes a flamethrower 361 disposed on one side of the inspection chamber 32 , a camera 362 disposed on the other side of the inspection chamber 32 , an air outlet pipe 363 and an air inlet pipe 364 connected to the interior of the inspection chamber 32 .

[0065] In this embodiment, the oxygen content in the inspection chamber 32 is adjusted by setting an air outlet pipe 363 and an air inlet pipe 364, and the flame gun 361 is used to check whether the halogen-free flame retardant continues to burn under qualified inspection values ​​of flame temperature and oxygen content. The inspection value is increased to allow the halogen-free flame retardant to continue to burn out, and the camera 362 is used to check whether the carbon film generated after the halogen-free flame retardant burns is dense and continuous, thereby checking whether the halogen-free flame retardant is qualified.

[0066] It should be noted that the air outlet pipe 363 and the air inlet pipe 364 respectively output and input the gas into the inspection chamber 32 through the negative pressure equipment. The negative pressure equipment itself and the installation method are both existing technologies, which are not drawn in the drawings and will not be described in detail here.

[0067] In addition, the mounting frame 351 is movable in the up and down directions and is arranged in the inspection chamber 32. The mounting frame 351 is provided with a limit rod 355 for limiting the rotation of the scraper 352. The mounting frame 351 moves up and down to control the scraper 352 to accurately scrape the halogen-free flame retardant on the inspection disk 34. At the same time, the limit rod 355 cooperates to make the scraper 352 and the inspection disk 34 rub against each other, so that the carbon film produced after combustion can be scraped off, and the carbon film is blown into the exhaust pipe through the air intake pipe 364 for discharge.

[0068] Furthermore, as shown in the figure, the packaging mechanism 4 includes a telescopic tube 41 connected to the discharge port 31 and capable of being extended and retracted up and down, and a conveying assembly 42 arranged below the discharge port 31 and used to position and convey the packaging barrel 43 to the position directly below the telescopic tube 41 .

[0069] In this embodiment, a telescopic rod is provided for discharging the material, thereby preventing bubbles from being generated when the halogen-free flame retardant is packaged.

[0070] In detail, when in use, the conveying component 42 positions and conveys the packaging barrel 43 to the bottom of the telescopic tube 41, and the telescopic tube 41 is able to extend into the packaging barrel 43 to discharge the material. Then the telescopic tube 41 gradually contracts during the discharging process to avoid bubbles generated by the gas wrapped by the halogen-free flame retardant during the discharging process, until the packaging barrel 43 is full.

[0071] It should be noted that the automatically retractable telescopic tube 41 and the conveying assembly 42 with positioning and conveying functions are both existing technologies and will not be described in detail here.

[0072] In the description of the present invention, it should be understood that the terms "front and back", "left and right", etc., indicating directions or positional relationships, are based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the equipment or components referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they cannot be understood as limitations on the invention.

[0073] Of course, in this technical solution, those skilled in the art should understand that the term "one" should be understood as "at least one" or "one or more", that is, in one embodiment, the number of an element may be one, while in another embodiment, the number of the element may be multiple, and the term "one" should not be understood as a limitation on the quantity.

[0074] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by a person skilled in the art based on the technical guidance of the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be based on the scope of protection of the claims.

Claims

1. A method for preparing a water-based environmentally friendly halogen-free flame retardant, characterized in that: The following steps are involved: Step 1: A treatment process in which raw materials, decabromodiphenylethane, antimony trioxide, ammonium polyphosphate, titanium dioxide, and water are added to a mixing mechanism to form a mixture A. The mixing mechanism guides the mixture A to flow in a directional manner while stirring the mixture A for grinding until the solid raw materials are fully ground and mixed into the water to form a pretreatment solution. Step 2: Mixing process, adding the raw acrylic emulsion and the thickener to the pretreatment solution in the mixing mechanism to form a mixture B, and the mixing mechanism guides the mixture B to flow in a directional manner for grinding while stirring the mixture B. During the grinding process, the mixing mechanism further guides the mixture B to flow in a directional manner to collect and remove bubbles until the solid raw material is fully ground and mixed into the pretreatment solution and the bubbles are completely collected and removed to form a halogen-free flame retardant.

2. The method for preparing a water-based environmentally friendly halogen-free flame retardant according to claim 1, characterized in that: The mixing mechanism includes a mixing tank with an open upper end, a grinding assembly arranged in the mixing tank, a defoaming assembly arranged on the grinding assembly, and a stirring assembly rotatably arranged in the mixing tank, and the stirring assembly is used to guide the solutions on both sides of the mixing tank to the grinding assembly.

3. The method for preparing a water-based environmentally friendly halogen-free flame retardant according to claim 2, characterized in that: The grinding assembly includes a support frame arranged in the mixing tank, two rotating rollers that are spaced apart and rotatably arranged on the support frame and form a first grinding zone between the two, two grinding rollers that are rotatably arranged on the support frame and respectively cooperate with the two rotating rollers to form two second grinding zones, and two guide plates that are opened and closed on the support frame and located between the two rotating rollers. The guide plates are used to further guide the solution on the inside and outside of the mixing tank guided by the stirring assembly into the two second grinding zones or the first grinding zone by opening or closing.

4. The method for preparing a water-based environmentally friendly halogen-free flame retardant according to claim 3, characterized in that: The debubble assembly includes a debubble channel formed through the rotating roller and the grinding roller, a screen arranged at the lower end of the debubble channel, a spiral plate arranged in the debubble channel, and a plurality of inflow holes arranged at the upper ends of the rotating roller and the grinding roller and extending through the corresponding debubble channels. The spiral plate is used to further guide the solution to flow to the screen to collect and remove bubbles while the rotating roller cooperates with the grinding roller to grind.

5. The method for preparing a water-based environmentally friendly halogen-free flame retardant according to claim 1, characterized in that: In the treatment process, the mixing mechanism first stirs at a low speed to preliminarily dissolve the solid raw materials in water to form a mixture A, then stirs at a high speed to increase the grinding speed of the solid raw materials in the mixture A, and finally stirs at a low speed to naturally expel the bubbles that have been stirred into the mixture A to form a pre-treated solution; In the mixing process, the mixing mechanism first stirs at a low speed to preliminarily dissolve the solid raw materials into the pretreatment solution to form a mixture B, then stirs at a high speed to increase the grinding speed of the solid raw materials in the mixture B, and finally stirs at a low speed to directionally collect and remove the bubbles that are quickly stirred into the mixture B to form a halogen-free flame retardant.

6. The method for preparing a water-based environmentally friendly halogen-free flame retardant according to claim 1, characterized in that: The method for preparing the water-based environmentally friendly halogen-free flame retardant further comprises the following steps: Step 3: Inspection process, sampling the halogen-free flame retardant formed in the mixing mechanism multiple times, and after inspecting whether the sample contains unmixed large particles, inspecting whether the combustion effect of the sample is qualified; Step 4: packaging process, the halogen-free flame retardant that has passed the inspection in the mixing mechanism is packaged.

7. The method for preparing a water-based environmentally friendly halogen-free flame retardant according to claim 6, characterized in that: In the inspection process, qualified inspection values ​​of flame temperature and oxygen content are set to inspect whether the halogen-free flame retardant continues to burn.

8. The method for preparing a water-based environmentally friendly halogen-free flame retardant according to claim 7, characterized in that: In the inspection process, the flame temperature and oxygen content are increased to allow the halogen-free flame retardant to burn out continuously, and whether the carbon film generated after the combustion of the halogen-free flame retardant is dense and continuous is detected.

9. A flame retardant obtained by the method for preparing a water-based, environmentally friendly, halogen-free flame retardant according to any one of claims 1 to 8, comprising: 12% decabromodiphenylethane, 4% antimony trioxide, 8% ammonium polyphosphate, 4% titanium dioxide, 30% acrylic emulsion, 2% thickener and 40% water.

10. A flame retardant according to claim 9, characterized in that: The thickener is bentonite, magnesium aluminum silicate, hydroxyethyl cellulose or carboxymethyl cellulose.

Citation Information

Patent Citations

  • Preparation method of halogen-free flame retardant, halogen-free flame retardant and sealant

    CN112876739A